#------------------------------------------------------------------------------ #$Date: 2025-03-04 21:28:44 +0200 (Tue, 04 Mar 2025) $ #$Revision: 298154 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573838.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1573838 loop_ _publ_author_name 'Zhu, Ming' 'Huang, Pei-Zhi' 'Li, Lin-Mei' 'Yang, Yi-Xuan' 'Pan, Lei' 'Wang, Zhi-Jie' 'Ni, Hao-Fei' 'Zhang, Feng-Wen' 'Teri, Gele' 'Zhang, Zhi-Xu' 'Liu, Zunqi' 'Fu, Da-Wei' 'Zhang, Yi' _publ_section_title ; Thermal-responsive luminescence/dielectric responses with reversibly shifted light emissions. ; _journal_issue 9 _journal_name_full 'Chemical science' _journal_page_first 4101 _journal_page_last 4108 _journal_paper_doi 10.1039/d4sc06631f _journal_volume 16 _journal_year 2025 _chemical_formula_moiety 'F6 P, C12 H24 O6, C6 H9 N2' _chemical_formula_sum 'C18 H33 F6 N2 O6 P' _chemical_formula_weight 518.43 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2024-08-20 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-08-20 deposited with the CCDC. 2025-01-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.634(18) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.985(5) _cell_length_b 10.522(3) _cell_length_c 19.813(7) _cell_measurement_reflns_used 5069 _cell_measurement_temperature 383.00 _cell_measurement_theta_max 55.044 _cell_measurement_theta_min 3.725 _cell_volume 2455.6(15) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 383.00 _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.960 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_av_unetI/netI 0.0548 _diffrn_reflns_Laue_measured_fraction_full 0.979 _diffrn_reflns_Laue_measured_fraction_max 0.960 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 21041 _diffrn_reflns_point_group_measured_fraction_full 0.979 _diffrn_reflns_point_group_measured_fraction_max 0.960 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.626 _diffrn_reflns_theta_min 4.012 _diffrn_source_current 1.1 _diffrn_source_power 0.05500000000000001 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.739 _exptl_absorpt_correction_T_max 0.7533 _exptl_absorpt_correction_T_min 0.5496 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1425 before and 0.0628 after correction. The Ratio of minimum to maximum transmission is 0.7296. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.402 _exptl_crystal_description block _exptl_crystal_F_000 1088 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.902 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.078 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 299 _refine_ls_number_reflns 4604 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.986 _refine_ls_R_factor_all 0.1736 _refine_ls_R_factor_gt 0.1179 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2357 _refine_ls_wR_factor_ref 0.2606 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2324 _reflns_number_total 4604 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc06631f2.cif _cod_data_source_block cu_zm_45_383k_5_0m_a _cod_depositor_comments 'Adding full bibliography for 1573833--1573838.cif.' _cod_original_cell_volume 2455.5(14) _cod_database_code 1573838 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.832 _shelx_estimated_absorpt_t_min 0.805 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C16(H16A,H16B), C18(H18A,H18B), C13(H13A,H13B) 2.b Aromatic/amide H refined with riding coordinates: C2(H2), C7(H7), C15(H15), C17(H17) 2.c Idealised Me refined as rotating group: N1(H1C,H1D,H1E) ; _shelx_res_file ; TITL cu_ZM_45_383K_5_0m_a.res in P2(1)/n cu_zm_45_383k_5_0m_a.res created by SHELXL-2018/3 at 15:48:01 on 20-Aug-2024 REM Old TITL Integration of ZM_45_383K_5 REM SHELXT solution in P2(1)/n: R1 0.273, Rweak 0.038, Alpha 0.067 REM 0.388 for 267 systematic absences, Orientation as input REM Formula found by SHELXT: C25 F2 N3 O4 P CELL 1.54184 11.9848 10.522 19.8126 90 100.634 90 ZERR 4 0.0046 0.0026 0.0069 0 0.018 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H F N O P UNIT 72 132 24 8 24 4 L.S. 20 PLAN 1 SIZE 0.11 0.12 0.13 TEMP 109.85 CONF FREE F2 F1 FREE F2 F4 FREE F5 F1 FREE F5 F3 LIST 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.020000 10.000000 FVAR 0.41363 P1 6 0.180127 0.793991 0.437236 11.00000 0.11395 0.08195 = 0.08417 -0.01035 0.01811 -0.00241 F1 3 0.208587 0.709611 0.385870 11.00000 0.18158 0.34674 = 0.46067 -0.28642 0.12643 -0.04498 F2 3 0.230948 0.901102 0.410744 11.00000 0.47846 0.28148 = 0.20610 0.00826 0.05676 -0.25619 F3 3 0.127693 0.686394 0.463160 11.00000 0.49605 0.26776 = 0.18979 0.10080 -0.05927 -0.24222 F4 3 0.284958 0.782750 0.483923 11.00000 0.33333 0.17030 = 0.49970 -0.02842 -0.29617 0.02272 F5 3 0.071880 0.804507 0.388100 11.00000 0.18617 0.18962 = 0.38812 -0.01693 -0.11539 0.03173 F6 3 0.154180 0.882639 0.485650 11.00000 0.41092 0.37182 = 0.31816 -0.24093 0.24284 -0.13449 O1 5 0.714198 0.512583 0.333149 11.00000 0.09058 0.08389 = 0.09976 0.01288 0.00989 0.01682 O2 5 0.493817 0.962548 0.254883 11.00000 0.12384 0.09220 = 0.13644 0.03905 0.04373 0.03109 O3 5 0.687753 0.691361 0.433683 11.00000 0.09364 0.11869 = 0.06966 0.00317 0.00317 -0.00737 O4 5 0.607109 0.932070 0.387182 11.00000 0.13904 0.08889 = 0.10209 -0.01966 0.04281 -0.00160 O5 5 0.593229 0.539223 0.202588 11.00000 0.09658 0.10656 = 0.07842 -0.01960 0.02408 -0.00684 O6 5 0.534380 0.785455 0.158680 11.00000 0.08522 0.14434 = 0.07437 0.01882 0.00005 -0.00613 C1 1 0.522418 1.064931 0.300167 11.00000 0.15944 0.07896 = 0.20694 0.01723 0.06888 0.03975 AFIX 23 H1A 2 0.468084 1.133227 0.287945 11.00000 -1.20000 H1B 2 0.597008 1.096709 0.296424 11.00000 -1.20000 AFIX 0 C4 1 0.736793 0.486179 0.403649 11.00000 0.11401 0.12922 = 0.10783 0.04212 0.01332 0.03837 AFIX 23 H4A 2 0.794105 0.420285 0.413414 11.00000 -1.20000 H4B 2 0.668367 0.456090 0.418073 11.00000 -1.20000 AFIX 0 C5 1 0.623992 0.896038 0.456551 11.00000 0.16520 0.11825 = 0.10146 -0.04663 0.05004 -0.04733 AFIX 23 H5A 2 0.555922 0.856262 0.466644 11.00000 -1.20000 H5B 2 0.641017 0.970132 0.485766 11.00000 -1.20000 AFIX 0 C6 1 0.588134 0.579906 0.133464 11.00000 0.12056 0.14997 = 0.07831 -0.03020 0.03249 -0.03253 AFIX 23 H6A 2 0.569155 0.508571 0.102460 11.00000 -1.20000 H6B 2 0.661458 0.612742 0.127774 11.00000 -1.20000 AFIX 0 C8 1 0.495314 0.994195 0.186525 11.00000 0.11823 0.13798 = 0.13144 0.07125 0.01944 0.04101 AFIX 23 H8A 2 0.571566 1.018829 0.181971 11.00000 -1.20000 H8B 2 0.445359 1.065958 0.173047 11.00000 -1.20000 AFIX 0 C9 1 0.522469 1.023746 0.372318 11.00000 0.18462 0.09922 = 0.17611 -0.02061 0.08180 0.02678 AFIX 23 H9A 2 0.538543 1.095167 0.403557 11.00000 -1.20000 H9B 2 0.449297 0.988309 0.376412 11.00000 -1.20000 AFIX 0 C10 1 0.667264 0.436881 0.220537 11.00000 0.10460 0.10085 = 0.13777 -0.04381 0.03291 -0.00270 AFIX 23 H10A 2 0.742051 0.458565 0.211931 11.00000 -1.20000 H10B 2 0.640030 0.363451 0.192716 11.00000 -1.20000 AFIX 0 C11 1 0.502184 0.678682 0.117342 11.00000 0.10049 0.19463 = 0.06236 0.00197 0.00109 -0.02679 AFIX 23 H11A 2 0.493722 0.702054 0.069306 11.00000 -1.20000 H11B 2 0.429715 0.647060 0.125335 11.00000 -1.20000 AFIX 0 C12 1 0.719468 0.805984 0.469345 11.00000 0.13696 0.16304 = 0.06767 -0.01178 0.01247 -0.05433 AFIX 23 H12A 2 0.784768 0.842436 0.453940 11.00000 -1.20000 H12B 2 0.740245 0.789103 0.518183 11.00000 -1.20000 AFIX 0 C14 1 0.776961 0.602009 0.441054 11.00000 0.10003 0.18446 = 0.09057 0.01760 -0.01197 0.02223 AFIX 23 H14A 2 0.802643 0.582595 0.489281 11.00000 -1.20000 H14B 2 0.840429 0.637097 0.423120 11.00000 -1.20000 AFIX 0 C16 1 0.458498 0.886534 0.141508 11.00000 0.09878 0.20574 = 0.10098 0.06352 0.00452 0.02129 AFIX 23 H16A 2 0.382818 0.860561 0.146562 11.00000 -1.20000 H16B 2 0.456055 0.910938 0.094046 11.00000 -1.20000 AFIX 0 C18 1 0.674245 0.406571 0.293040 11.00000 0.09759 0.07279 = 0.15596 0.00021 0.02571 0.01434 AFIX 23 H18A 2 0.599828 0.382681 0.301425 11.00000 -1.20000 H18B 2 0.725255 0.335318 0.305466 11.00000 -1.20000 AFIX 0 N1 4 0.543922 0.713063 0.301224 11.00000 0.07564 0.06565 = 0.06391 0.00386 0.01432 0.00558 AFIX 137 H1C 2 0.560368 0.662794 0.268281 11.00000 -1.20000 H1D 2 0.589161 0.694261 0.340840 11.00000 -1.20000 H1E 2 0.554266 0.793824 0.290525 11.00000 -1.20000 AFIX 0 N2 4 0.357157 0.314690 0.354978 11.00000 0.12058 0.09141 = 0.21460 -0.00225 0.07374 -0.01189 C2 1 0.338156 0.354087 0.293250 11.00000 0.09039 0.13043 = 0.15757 -0.04845 0.03694 -0.02434 AFIX 43 H2 2 0.307866 0.297059 0.258856 11.00000 -1.20000 AFIX 0 C3 1 0.401507 0.560911 0.323530 11.00000 0.06409 0.07723 = 0.08614 -0.00254 0.02449 0.00376 C7 1 0.420209 0.518423 0.389306 11.00000 0.11165 0.09971 = 0.09170 -0.00265 0.03461 -0.00153 AFIX 43 H7 2 0.449022 0.572854 0.425299 11.00000 -1.20000 AFIX 0 C13 1 0.425219 0.693800 0.307860 11.00000 0.07584 0.09079 = 0.12910 0.02603 0.03464 0.01914 AFIX 23 H13A 2 0.376113 0.718507 0.265331 11.00000 -1.20000 H13B 2 0.407930 0.748159 0.344112 11.00000 -1.20000 AFIX 0 C15 1 0.359906 0.476803 0.274271 11.00000 0.08177 0.14328 = 0.09796 -0.00604 0.02207 -0.00494 AFIX 43 H15 2 0.345997 0.500643 0.228281 11.00000 -1.20000 AFIX 0 C17 1 0.396469 0.395998 0.401929 11.00000 0.16201 0.11049 = 0.13678 0.03186 0.06315 0.00500 AFIX 43 H17 2 0.409351 0.368846 0.447376 11.00000 -1.20000 AFIX 0 HKLF 4 REM cu_ZM_45_383K_5_0m_a.res in P2(1)/n REM wR2 = 0.2606, GooF = S = 0.986, Restrained GooF = 0.986 for all data REM R1 = 0.1179 for 2324 Fo > 4sig(Fo) and 0.1736 for all 4604 data REM 299 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.902, deepest hole -0.617, 1-sigma level 0.078 Q1 1 0.1568 0.9285 0.4431 11.00000 0.05 0.90 ; _shelx_res_checksum 33361 _shelx_hkl_file ; 1 0 0 0.81 0.79 2 0 0 11.12 0.92 2 0 0 11.45 2.31 -2 0 0 11.72 0.83 -2 0 0 9.66 2.23 -2 0 0 9.38 0.75 2 0 0 10.42 0.80 -3 0 0 0.06 2.89 -3 0 0 -0.22 0.27 3 0 0 0.13 0.31 3 0 0 -0.41 2.70 3 0 0 0.55 0.40 -3 0 0 0.98 0.43 -4 0 0 2.49 4.13 4 0 0 2.06 0.56 -4 0 0 1.07 0.61 4 0 0 1.04 4.08 -4 0 0 1.20 0.37 4 0 0 2.11 0.51 -5 0 0 6.69 7.72 6 0 0 34.11 2.84 -6 0 0 38.58 3.17 6 0 0 39.36 3.03 -6 0 0 36.99 12.55 -6 0 0 59.15 21.37 -7 0 0 5.74 32.22 7 0 0 -0.33 0.30 7 0 0 -0.31 1.60 -7 0 0 -0.02 0.89 7 0 0 0.28 0.43 -8 0 0 74.16 6.10 -8 0 0 71.68 5.66 8 0 0 77.67 4.87 9 0 0 0.05 0.47 -9 0 0 0.00 1.46 -9 0 0 -0.03 0.96 -10 0 0 9.65 2.12 10 0 0 13.61 1.40 -10 0 0 18.21 3.11 -11 0 0 -1.06 0.96 11 0 0 0.53 0.56 -11 0 0 0.39 1.43 -12 0 0 0.91 1.47 -12 0 0 1.28 1.21 -13 0 0 -0.46 0.83 -13 0 0 -0.62 1.13 -14 0 0 0.31 0.85 -14 0 0 0.92 0.74 0 -1 0 0.06 0.12 0 -1 0 0.13 0.09 0 -1 0 -0.04 0.07 0 -1 0 -0.79 1.19 0 1 0 -0.73 1.18 0 1 0 0.06 0.06 0 1 0 0.05 0.09 1 -1 0 212.21 12.70 1 -1 0 213.21 12.59 -1 -1 0 207.26 12.51 -1 -1 0 197.35 13.22 -1 1 0 228.33 13.65 1 1 0 208.07 13.05 1 1 0 218.36 12.51 2 -1 0 4217.51 258.07 -2 -1 0 4183.86 257.67 2 1 0 4372.94 257.41 -2 1 0 4656.69 258.22 -3 -1 0 4388.78 254.06 3 -1 0 3996.47 254.20 3 1 0 4135.98 253.50 -3 1 0 4603.26 254.57 4 -1 0 167.51 10.48 -4 -1 0 171.50 10.23 4 -1 0 172.14 10.26 -4 -1 0 169.68 14.18 -4 1 0 175.69 14.27 4 1 0 168.59 10.15 4 1 0 166.59 10.21 4 1 0 161.44 10.05 4 1 0 164.70 13.03 5 -1 0 275.16 16.51 -5 -1 0 274.58 16.52 5 -1 0 273.12 16.74 5 -1 0 284.20 16.51 -5 -1 0 276.34 22.42 5 1 0 275.49 16.38 5 1 0 269.37 16.44 5 1 0 236.85 20.37 -5 1 0 301.56 30.65 5 1 0 255.92 16.24 -5 1 0 305.52 23.37 6 -1 0 86.78 6.09 6 -1 0 99.56 6.25 6 -1 0 90.97 5.68 -6 -1 0 93.32 16.20 -6 -1 0 81.62 6.23 -6 1 0 114.62 24.05 -6 1 0 110.83 17.04 -6 1 0 92.90 6.37 7 -1 0 96.40 5.84 -7 -1 0 95.49 6.48 -7 -1 0 69.90 32.02 7 -1 0 81.50 6.72 -7 1 0 44.56 35.20 7 1 0 94.94 5.75 -7 1 0 146.98 25.94 -7 1 0 87.80 6.53 -8 -1 0 23.36 2.58 8 -1 0 18.07 2.15 -8 -1 0 20.47 3.01 8 -1 0 23.48 1.87 -8 1 0 21.37 2.62 8 1 0 22.43 1.75 -8 1 0 31.02 3.63 9 -1 0 10.52 1.55 -9 -1 0 15.37 2.75 -9 -1 0 10.60 2.09 9 -1 0 13.95 1.41 -9 1 0 15.53 2.75 9 1 0 12.02 1.28 -9 1 0 13.58 2.37 10 -1 0 0.17 0.53 -10 -1 0 -0.08 1.13 -10 -1 0 -0.41 1.53 -10 1 0 0.47 1.57 -10 1 0 0.41 1.12 10 1 0 1.36 0.57 -11 -1 0 5.12 1.75 -11 -1 0 5.19 1.91 11 -1 0 6.23 1.01 -11 1 0 6.92 2.17 -11 1 0 5.05 1.66 11 1 0 6.67 0.92 -12 -1 0 0.33 1.03 -12 -1 0 2.48 1.67 -12 1 0 -0.22 1.25 -12 1 0 0.73 1.06 -13 -1 0 1.52 1.31 -13 -1 0 0.60 0.99 -13 1 0 1.27 1.26 -13 1 0 0.63 0.92 -14 -1 0 -0.45 0.58 -14 -1 0 0.87 1.00 -14 1 0 1.19 1.19 -14 1 0 -0.33 0.86 0 -2 0 51.88 3.25 0 -2 0 53.96 5.81 0 -2 0 50.33 3.14 0 2 0 51.37 3.10 0 2 0 51.48 3.14 0 2 0 54.77 5.78 1 -2 0 1062.68 64.04 -1 -2 0 1156.05 65.17 -1 -2 0 1103.13 63.92 1 -2 0 1097.97 64.03 1 2 0 1111.59 63.93 1 2 0 975.88 64.84 -1 2 0 1090.77 66.83 -2 -2 0 488.23 35.21 2 -2 0 565.91 33.92 2 -2 0 567.44 33.91 -2 -2 0 569.59 33.77 2 2 0 598.20 33.77 -2 2 0 588.72 38.24 2 2 0 606.74 34.69 -2 2 0 596.76 36.12 3 -2 0 7.57 0.66 -3 -2 0 7.88 0.74 3 -2 0 7.99 1.16 3 -2 0 8.08 0.94 3 -2 0 6.18 0.86 -3 -2 0 10.15 4.17 3 2 0 7.75 0.68 -3 2 0 6.75 7.99 3 2 0 5.70 2.63 3 2 0 7.23 0.55 -3 2 0 5.38 4.04 4 -2 0 19.97 1.75 4 -2 0 19.81 1.93 4 -2 0 21.53 1.49 -4 -2 0 13.25 6.66 -4 -2 0 21.57 1.65 4 -2 0 19.99 1.72 -4 2 0 17.48 10.83 -4 2 0 26.78 7.50 4 2 0 20.57 1.35 4 2 0 20.27 1.50 4 2 0 17.56 4.57 -5 -2 0 18.98 9.70 5 -2 0 17.74 1.89 5 -2 0 15.30 1.82 5 -2 0 16.69 1.94 5 -2 0 16.70 1.32 -5 -2 0 17.03 1.80 5 2 0 17.45 1.50 -5 2 0 22.19 3.24 -5 2 0 18.82 9.08 5 2 0 16.60 1.19 -5 2 0 9.53 15.71 6 -2 0 69.34 4.98 6 -2 0 66.14 4.96 -6 -2 0 52.17 16.54 6 -2 0 65.46 4.33 -6 -2 0 75.90 21.88 -6 2 0 87.17 16.88 6 2 0 67.99 4.57 -6 2 0 66.01 5.01 -6 2 0 47.79 27.68 7 -2 0 90.05 6.96 7 -2 0 91.45 6.37 7 -2 0 85.45 5.66 -7 -2 0 89.90 6.21 -7 -2 0 63.19 34.89 -7 2 0 120.96 43.06 7 2 0 92.08 5.52 -7 2 0 84.69 6.42 -7 2 0 143.52 30.08 -7 2 0 82.28 6.83 8 -2 0 171.69 11.55 -8 -2 0 185.15 12.02 8 -2 0 190.53 11.38 -8 -2 0 181.62 12.59 8 2 0 195.09 11.19 -8 2 0 173.03 12.16 -8 2 0 187.49 12.54 9 -2 0 1.53 0.66 9 -2 0 2.18 1.01 -9 -2 0 0.20 1.67 -9 -2 0 2.44 1.26 9 -2 0 -0.34 0.66 9 2 0 2.41 0.57 -9 2 0 2.22 1.32 -9 2 0 1.90 1.64 10 -2 0 11.91 1.65 -10 -2 0 13.26 2.30 -10 -2 0 13.81 2.82 10 -2 0 14.95 1.60 10 2 0 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220.95 13.14 4 -4 0 219.47 13.41 4 -4 0 207.80 13.42 4 -4 0 211.32 13.26 -4 4 0 247.20 30.68 5 -4 0 311.71 18.71 5 -4 0 300.59 18.40 5 -4 0 295.16 18.05 5 -4 0 297.25 17.90 -5 -4 0 294.66 24.12 5 -4 0 312.11 18.31 -5 -4 0 228.18 24.73 -5 4 0 302.09 41.96 6 -4 0 1.10 0.92 6 -4 0 0.44 0.90 6 -4 0 1.15 0.84 -6 -4 0 -30.69 17.28 6 -4 0 0.03 2.36 6 -4 0 -0.79 2.79 6 -4 0 0.73 0.52 -6 4 0 -68.34 50.16 -6 4 0 38.52 27.94 -6 4 0 -0.10 0.85 -6 4 0 0.25 1.27 6 4 0 0.27 0.21 6 4 0 0.35 0.21 7 -4 0 52.10 4.56 7 -4 0 54.98 3.76 7 -4 0 53.58 3.92 7 -4 0 54.14 4.05 -7 -4 0 55.64 4.12 7 4 0 54.18 3.28 7 4 0 54.52 3.28 -7 4 0 43.47 4.16 -7 4 0 54.85 4.87 8 -4 0 -0.84 0.65 8 -4 0 -0.62 0.40 8 -4 0 -0.84 0.88 -8 -4 0 0.08 0.94 8 -4 0 -0.28 0.94 -8 4 0 -0.51 1.32 8 4 0 0.07 0.20 -8 4 0 0.28 1.05 8 4 0 0.35 0.19 9 -4 0 9.53 1.43 9 -4 0 13.54 1.89 -9 -4 0 13.03 2.11 -9 4 0 9.14 2.31 -9 4 0 10.82 2.08 -10 -4 0 1.64 1.89 -10 -4 0 1.20 1.10 10 -4 0 -1.43 0.89 10 -4 0 0.66 0.84 10 -4 0 1.34 0.94 -10 4 0 0.51 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-20 0.45 0.68 1 -7 -20 1.27 0.70 0 -7 -20 1.14 0.64 9 0 -21 1.16 0.52 8 0 -21 -0.28 0.53 7 0 -21 4.14 0.99 6 0 -21 -0.42 0.67 5 0 -21 0.39 0.81 4 0 -21 0.27 0.96 4 0 -21 1.13 0.46 3 0 -21 0.05 1.01 3 0 -21 -0.60 0.88 2 0 -21 0.17 0.86 2 0 -21 -0.76 0.98 1 0 -21 0.74 1.11 1 0 -21 0.72 1.14 0 0 -21 0.53 1.13 0 0 -21 -0.96 0.93 -1 0 -21 0.66 1.12 -1 0 -21 -0.47 0.93 -2 0 -21 0.33 0.78 -2 0 -21 -1.25 0.95 -3 0 -21 3.06 1.14 -3 0 -21 1.72 0.87 -4 0 -21 -0.14 0.82 -4 0 -21 -0.31 0.57 9 -1 -21 -0.15 0.45 -8 -1 21 -0.18 0.64 8 -1 -21 0.02 0.58 8 1 -21 -0.44 0.49 -7 -1 21 0.10 0.64 7 -1 -21 1.13 0.77 7 1 -21 -0.55 0.59 -6 -1 21 -1.47 0.57 6 -1 -21 0.51 0.83 6 1 -21 0.00 0.73 5 -1 -21 0.13 0.55 5 -1 -21 0.18 0.84 5 1 -21 -0.67 0.73 4 -1 -21 0.04 0.84 4 -1 -21 -1.14 0.91 4 1 -21 -0.88 0.76 3 -1 -21 8.60 1.63 3 -1 -21 6.40 1.39 3 1 -21 10.78 1.75 2 -1 -21 -1.07 0.85 2 -1 -21 -1.76 1.03 2 1 -21 -0.56 0.83 2 1 -21 0.98 0.66 1 -1 -21 -0.05 1.01 1 -1 -21 0.09 1.14 1 1 -21 -0.86 0.88 1 1 -21 0.22 0.98 0 -1 -21 0.00 1.07 0 -1 -21 -0.43 0.88 0 1 -21 0.60 1.02 0 1 -21 -0.07 0.96 -1 -1 -21 0.46 1.07 -1 -1 -21 -0.58 0.83 -1 1 -21 0.12 0.94 -1 1 -21 0.04 0.96 -2 -1 -21 0.55 0.90 -2 -1 -21 -0.56 0.96 -2 1 -21 0.63 0.80 -2 1 -21 -0.13 0.91 -3 -1 -21 1.74 0.89 -3 -1 -21 0.30 0.97 -3 1 -21 0.66 0.75 -3 1 -21 -0.08 0.86 -4 -1 -21 0.94 0.96 -4 -1 -21 0.11 0.59 -4 1 -21 1.51 0.83 -4 1 -21 -0.95 0.53 9 -2 -21 0.18 0.45 -9 -2 21 0.18 0.55 -8 -2 21 -0.38 0.65 8 -2 -21 -0.17 0.54 8 2 -21 -0.33 0.31 7 -2 -21 2.43 0.87 -7 -2 21 1.03 0.77 7 2 -21 0.87 0.63 6 -2 -21 0.03 0.72 6 -2 -21 0.34 0.44 6 2 -21 0.02 0.69 5 -2 -21 2.39 1.01 5 -2 -21 4.15 1.16 5 2 -21 3.03 1.02 4 -2 -21 0.21 0.91 4 -2 -21 1.53 1.08 4 2 -21 -0.86 0.74 3 -2 -21 -0.39 0.82 3 -2 -21 -0.43 1.05 3 2 -21 -0.19 0.79 2 -2 -21 -0.18 0.84 2 -2 -21 -0.76 1.09 2 2 -21 0.00 0.84 1 -2 -21 4.16 1.40 1 -2 -21 5.91 1.36 1 2 -21 5.20 1.40 0 -2 -21 -1.39 1.01 0 -2 -21 0.63 0.86 0 2 -21 0.58 0.91 0 2 -21 3.60 0.88 -1 -2 -21 -1.60 0.94 -1 -2 -21 -1.10 0.69 -1 2 -21 -0.03 0.83 -2 -2 -21 0.24 0.97 -2 -2 -21 0.10 0.74 -2 2 -21 0.21 0.72 -2 2 -21 1.36 0.56 -3 -2 -21 -0.52 0.78 -3 -2 -21 0.74 0.69 -3 2 -21 0.10 0.65 -4 -2 -21 0.27 0.76 -4 -2 -21 0.51 0.62 -4 2 -21 -0.09 0.58 -8 -3 21 0.17 0.58 8 -3 -21 -0.05 0.51 7 -3 -21 0.18 0.60 6 -3 -21 0.22 0.78 6 -3 -21 0.74 0.73 6 3 -21 0.33 0.60 5 -3 -21 -1.07 0.67 5 -3 -21 -0.66 0.87 5 3 -21 0.39 0.71 4 -3 -21 -0.49 0.68 4 -3 -21 0.25 1.00 4 3 -21 0.46 0.78 3 -3 -21 1.28 0.91 3 -3 -21 0.28 1.04 3 3 -21 1.66 0.92 2 -3 -21 0.70 0.86 2 -3 -21 0.79 1.04 2 3 -21 -0.30 0.77 1 -3 -21 0.35 0.82 1 -3 -21 0.59 1.13 1 3 -21 -0.65 0.69 0 -3 -21 0.68 1.01 0 -3 -21 1.37 0.85 0 3 -21 0.32 0.82 -1 -3 -21 0.22 0.98 -1 -3 -21 0.32 0.75 -1 3 -21 -0.35 0.72 -2 -3 -21 0.16 0.97 -2 -3 -21 -0.10 0.65 -2 3 -21 -0.07 0.72 -3 -3 -21 0.33 0.58 -3 -3 -21 -0.50 0.76 -3 3 -21 0.07 0.63 -4 -3 -21 -0.22 0.67 -4 3 -21 -0.34 0.46 8 -4 -21 0.59 0.49 -8 -4 21 0.84 0.67 7 -4 -21 0.03 0.53 6 -4 -21 0.80 0.79 6 -4 -21 0.21 0.60 5 -4 -21 -0.07 0.86 5 -4 -21 0.27 0.69 5 4 -21 0.09 0.35 4 -4 -21 -0.23 0.89 4 -4 -21 -0.08 0.68 4 4 -21 0.16 0.62 3 -4 -21 1.44 0.83 3 -4 -21 0.32 0.99 3 4 -21 1.21 0.74 2 -4 -21 0.96 0.74 2 -4 -21 1.18 1.02 2 4 -21 0.76 0.73 1 -4 -21 -1.03 0.87 1 -4 -21 -0.50 0.64 1 4 -21 -0.43 0.62 0 -4 -21 0.66 0.67 0 -4 -21 -0.36 0.90 0 4 -21 0.13 0.70 -1 -4 -21 0.42 0.68 -1 -4 -21 0.26 0.94 -1 4 -21 -0.82 0.59 -2 -4 -21 0.25 0.80 -2 4 -21 0.55 0.65 -3 -4 -21 0.87 0.76 -3 4 -21 -0.07 0.55 6 -5 -21 -0.19 0.66 6 -5 -21 0.31 0.55 5 -5 -21 0.50 0.78 5 -5 -21 -0.07 0.54 4 -5 -21 0.29 0.82 4 -5 -21 0.07 0.57 3 -5 -21 -0.16 0.55 3 -5 -21 0.28 0.85 3 5 -21 0.36 0.38 2 -5 -21 -0.31 0.80 2 -5 -21 -0.17 0.58 2 5 -21 -0.65 0.48 1 -5 -21 0.14 0.60 1 -5 -21 0.52 0.86 1 5 -21 0.27 0.56 0 -5 -21 0.40 0.73 0 5 -21 -0.47 0.51 -1 -5 -21 1.59 0.84 -1 5 -21 0.68 0.53 -2 -5 -21 -0.55 0.63 -2 5 -21 -0.16 0.45 5 -6 -21 0.24 0.63 5 -6 -21 -0.62 0.38 4 -6 -21 0.84 0.70 4 -6 -21 0.26 0.45 3 -6 -21 -0.46 0.44 3 -6 -21 0.25 0.68 2 -6 -21 0.71 0.72 1 -6 -21 -0.09 0.66 0 -6 -21 0.34 0.66 8 0 -22 -0.53 0.42 7 0 -22 -0.18 0.50 6 0 -22 0.98 0.74 5 0 -22 -0.71 0.72 4 0 -22 0.96 0.78 3 0 -22 -1.00 0.70 3 0 -22 1.41 0.54 2 0 -22 0.92 0.88 2 0 -22 1.54 0.96 1 0 -22 -0.35 0.75 1 0 -22 0.42 0.96 0 0 -22 8.37 1.49 -1 0 -22 0.52 0.79 -1 0 -22 -0.16 0.91 -2 0 -22 -1.09 0.75 -2 0 -22 -0.29 0.68 -3 0 -22 -0.53 0.55 -3 0 -22 0.08 0.73 8 -1 -22 1.54 0.59 8 1 -22 1.15 0.45 7 -1 -22 -0.17 0.57 7 1 -22 -0.21 0.50 6 -1 -22 0.57 0.73 6 1 -22 0.32 0.65 5 -1 -22 -0.16 0.69 5 1 -22 0.27 0.69 4 -1 -22 1.52 0.95 4 -1 -22 1.23 0.81 4 1 -22 0.63 0.82 3 -1 -22 -1.12 0.80 3 -1 -22 0.35 0.74 3 1 -22 0.80 0.82 2 -1 -22 0.35 0.97 2 -1 -22 0.40 0.85 2 1 -22 -0.17 0.71 1 -1 -22 1.66 1.12 1 -1 -22 -0.18 0.76 1 1 -22 2.67 0.56 1 1 -22 0.72 0.85 0 -1 -22 0.78 1.04 0 -1 -22 1.12 0.85 0 1 -22 -0.32 0.75 0 1 -22 2.52 0.85 -1 -1 -22 -1.36 0.61 -1 -1 -22 -0.85 0.86 -1 1 -22 -1.44 0.57 -1 1 -22 0.17 0.76 -2 -1 -22 1.79 0.79 -2 -1 -22 1.20 0.95 -2 1 -22 -0.03 0.68 -2 1 -22 2.03 0.82 -3 -1 -22 0.00 0.54 -3 -1 -22 0.05 0.77 -3 1 -22 -0.63 0.54 8 -2 -22 0.47 0.48 7 -2 -22 0.25 0.60 7 2 -22 0.04 0.43 6 -2 -22 4.12 0.92 -6 -2 22 -2.21 0.94 6 2 -22 3.67 0.78 5 -2 -22 1.77 0.79 5 -2 -22 1.84 0.84 5 2 -22 1.84 0.81 4 -2 -22 -0.08 0.84 4 -2 -22 -0.38 0.64 4 2 -22 -0.34 0.66 3 -2 -22 -0.45 0.92 3 -2 -22 0.30 0.75 3 2 -22 -0.66 0.65 2 -2 -22 0.67 0.77 2 -2 -22 -0.42 0.91 2 2 -22 -0.03 0.73 1 -2 -22 0.16 0.77 1 -2 -22 -0.53 0.95 1 2 -22 -0.37 0.65 0 -2 -22 3.55 1.13 0 -2 -22 4.90 1.10 0 2 -22 2.10 0.91 -1 -2 -22 1.64 0.80 -1 -2 -22 0.77 1.02 -1 2 -22 0.52 0.72 -2 -2 -22 0.27 0.58 -2 -2 -22 -0.43 0.78 -2 2 -22 -0.18 0.62 -3 -2 -22 -0.42 0.50 -3 -2 -22 0.50 0.66 -3 2 -22 -0.25 0.52 -7 -3 22 1.55 0.64 7 -3 -22 0.68 0.58 6 -3 -22 0.29 0.65 6 3 -22 0.30 0.39 5 -3 -22 1.72 0.75 5 -3 -22 1.24 0.77 5 3 -22 1.01 0.60 4 -3 -22 -0.68 0.64 4 -3 -22 -0.32 0.82 4 3 -22 -0.25 0.54 3 -3 -22 1.95 0.86 3 -3 -22 0.95 0.96 3 3 -22 1.16 0.73 2 -3 -22 -0.47 0.65 2 -3 -22 0.68 0.96 2 3 -22 -0.24 0.61 1 -3 -22 4.86 1.21 1 -3 -22 3.34 0.94 1 3 -22 3.51 0.97 0 -3 -22 0.81 0.68 0 -3 -22 0.34 0.87 0 3 -22 1.08 0.72 -1 -3 -22 -0.35 0.56 -1 -3 -22 -0.07 0.79 -1 3 -22 -0.24 0.60 -2 -3 -22 1.47 0.85 -2 -3 -22 0.15 0.54 -2 3 -22 0.22 0.60 6 -4 -22 0.13 0.50 5 -4 -22 0.91 0.75 5 -4 -22 1.04 0.64 4 -4 -22 1.22 0.66 4 -4 -22 0.07 0.79 4 4 -22 0.43 0.45 3 -4 -22 -0.63 0.74 3 -4 -22 0.05 0.57 3 4 -22 0.39 0.55 2 -4 -22 0.89 0.66 2 -4 -22 -0.02 0.78 2 4 -22 0.27 0.56 1 -4 -22 -0.02 0.55 1 -4 -22 0.22 0.80 1 4 -22 0.72 0.60 0 -4 -22 -0.15 0.72 0 -4 -22 1.81 0.63 0 4 -22 0.70 0.59 -1 -4 -22 2.39 0.84 -1 4 -22 1.17 0.60 4 -5 -22 -0.04 0.45 4 -5 -22 -0.57 0.60 3 -5 -22 0.18 0.44 3 -5 -22 0.42 0.70 2 -5 -22 0.05 0.68 2 -5 -22 -0.36 0.46 1 -5 -22 2.31 0.80 0 -5 -22 0.14 0.61 7 0 -23 0.73 0.47 6 0 -23 -0.44 0.52 5 0 -23 -0.03 0.59 4 0 -23 0.00 0.65 3 0 -23 0.09 0.65 2 0 -23 -1.38 0.55 1 0 -23 2.70 0.81 1 0 -23 0.90 0.72 0 0 -23 0.52 0.71 0 0 -23 1.19 0.72 -1 0 -23 2.22 1.02 -1 0 -23 -0.21 0.51 -2 0 -23 0.14 0.53 7 -1 -23 0.52 0.49 7 1 -23 -0.09 0.40 6 -1 -23 -0.14 0.53 6 1 -23 0.25 0.52 5 -1 -23 1.96 0.74 5 1 -23 3.65 0.83 4 -1 -23 -0.14 0.65 4 1 -23 0.53 0.60 3 -1 -23 0.18 0.67 3 -1 -23 0.35 0.68 3 1 -23 0.21 0.63 2 -1 -23 -0.87 0.54 2 -1 -23 0.18 0.71 2 1 -23 -0.12 0.60 1 -1 -23 1.05 0.76 1 -1 -23 1.07 0.86 1 1 -23 0.25 0.66 0 -1 -23 -0.26 0.73 0 -1 -23 0.57 0.63 0 1 -23 0.10 0.63 -1 -1 -23 2.99 0.91 -1 -1 -23 0.57 0.61 -1 1 -23 0.95 0.63 6 -2 -23 0.35 0.52 6 2 -23 0.20 0.40 5 -2 -23 0.11 0.57 5 2 -23 1.29 0.58 4 -2 -23 0.49 0.68 4 -2 -23 0.24 0.60 4 2 -23 0.26 0.55 3 -2 -23 0.05 0.60 3 -2 -23 0.60 0.74 3 2 -23 -0.24 0.58 2 -2 -23 0.12 0.79 2 -2 -23 -0.10 0.58 2 2 -23 0.32 0.62 1 -2 -23 1.20 0.87 1 -2 -23 -0.22 0.60 1 2 -23 -0.34 0.58 0 -2 -23 -0.04 0.75 0 -2 -23 -0.42 0.54 0 2 -23 -0.42 0.51 -1 -2 -23 0.66 0.54 -1 -2 -23 0.14 0.71 -1 2 -23 0.07 0.54 5 -3 -23 -0.02 0.52 5 3 -23 0.46 0.44 4 -3 -23 0.39 0.57 4 -3 -23 1.52 0.80 4 3 -23 0.14 0.48 3 -3 -23 0.60 0.74 3 -3 -23 -0.12 0.55 3 3 -23 0.20 0.49 2 -3 -23 1.32 0.81 2 -3 -23 1.00 0.63 2 3 -23 0.00 0.53 1 -3 -23 -0.15 0.50 1 -3 -23 0.47 0.73 1 3 -23 0.22 0.54 0 -3 -23 -0.35 0.65 0 -3 -23 0.19 0.50 0 3 -23 -0.16 0.46 3 -4 -23 -0.21 0.43 3 -4 -23 -0.01 0.57 2 -4 -23 -0.29 0.43 2 -4 -23 0.48 0.60 2 4 -23 0.27 0.40 1 -4 -23 1.79 0.73 4 0 -24 -0.07 0.48 3 0 -24 -0.50 0.43 2 0 -24 1.90 0.65 1 0 -24 -0.25 0.47 4 -1 -24 1.90 0.66 4 1 -24 1.22 0.55 3 -1 -24 -0.25 0.46 3 1 -24 0.12 0.50 2 -1 -24 0.78 0.59 2 1 -24 -0.23 0.45 1 -1 -24 -0.15 0.46 1 1 -24 -0.40 0.45 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 52339 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.18013(9) 0.79399(10) 0.43724(5) 0.0934(3) Uani 1 1 d . . . . . F1 F 0.2086(3) 0.7096(4) 0.3859(2) 0.3211(17) Uani 1 1 d . . . . . F2 F 0.2309(4) 0.9011(4) 0.4107(2) 0.323(2) Uani 1 1 d . . . . . F3 F 0.1277(4) 0.6864(4) 0.46316(19) 0.333(2) Uani 1 1 d . . . . . F4 F 0.2850(3) 0.7827(4) 0.4839(2) 0.382(2) Uani 1 1 d . . . . . F5 F 0.0719(3) 0.8045(4) 0.3881(2) 0.276(2) Uani 1 1 d . . . . . F6 F 0.1542(4) 0.8826(4) 0.48565(18) 0.3446(19) Uani 1 1 d . . . . . O1 O 0.71420(19) 0.5126(2) 0.33315(11) 0.0924(8) Uani 1 1 d . . . . . O2 O 0.4938(2) 0.9625(2) 0.25488(13) 0.1150(9) Uani 1 1 d . . . . . O3 O 0.68775(19) 0.6914(2) 0.43368(11) 0.0955(8) Uani 1 1 d . . . . . O4 O 0.6071(2) 0.9321(2) 0.38718(12) 0.1074(9) Uani 1 1 d . . . . . O5 O 0.59323(19) 0.5392(2) 0.20259(10) 0.0928(8) Uani 1 1 d . . . . . O6 O 0.53438(19) 0.7855(3) 0.15868(11) 0.1032(9) Uani 1 1 d . . . . . C1 C 0.5224(4) 1.0649(4) 0.3002(2) 0.1440(19) Uani 1 1 d . . . . . H1A H 0.468084 1.133227 0.287945 0.173 Uiso 1 1 calc R U . . . H1B H 0.597008 1.096709 0.296424 0.173 Uiso 1 1 calc R U . . . C4 C 0.7368(3) 0.4862(4) 0.40365(19) 0.1179(15) Uani 1 1 d . . . . . H4A H 0.794105 0.420285 0.413414 0.142 Uiso 1 1 calc R U . . . H4B H 0.668367 0.456090 0.418073 0.142 Uiso 1 1 calc R U . . . C5 C 0.6240(4) 0.8960(4) 0.45655(18) 0.1251(15) Uani 1 1 d . . . . . H5A H 0.555922 0.856262 0.466644 0.150 Uiso 1 1 calc R U . . . H5B H 0.641017 0.970132 0.485766 0.150 Uiso 1 1 calc R U . . . C6 C 0.5881(3) 0.5799(4) 0.13346(17) 0.1145(15) Uani 1 1 d . . . . . H6A H 0.569155 0.508571 0.102460 0.137 Uiso 1 1 calc R U . . . H6B H 0.661458 0.612742 0.127774 0.137 Uiso 1 1 calc R U . . . C8 C 0.4953(4) 0.9942(4) 0.1865(2) 0.1297(16) Uani 1 1 d . . . . . H8A H 0.571566 1.018829 0.181971 0.156 Uiso 1 1 calc R U . . . H8B H 0.445359 1.065958 0.173047 0.156 Uiso 1 1 calc R U . . . C9 C 0.5225(4) 1.0237(4) 0.3723(2) 0.1471(18) Uani 1 1 d . . . . . H9A H 0.538543 1.095167 0.403557 0.177 Uiso 1 1 calc R U . . . H9B H 0.449297 0.988309 0.376412 0.177 Uiso 1 1 calc R U . . . C10 C 0.6673(3) 0.4369(4) 0.2205(2) 0.1131(14) Uani 1 1 d . . . . . H10A H 0.742051 0.458565 0.211931 0.136 Uiso 1 1 calc R U . . . H10B H 0.640030 0.363451 0.192716 0.136 Uiso 1 1 calc R U . . . C11 C 0.5022(3) 0.6787(4) 0.11734(17) 0.1209(17) Uani 1 1 d . . . . . H11A H 0.493722 0.702054 0.069306 0.145 Uiso 1 1 calc R U . . . H11B H 0.429715 0.647060 0.125335 0.145 Uiso 1 1 calc R U . . . C12 C 0.7195(3) 0.8060(4) 0.46935(18) 0.1234(16) Uani 1 1 d . . . . . H12A H 0.784768 0.842436 0.453940 0.148 Uiso 1 1 calc R U . . . H12B H 0.740245 0.789103 0.518183 0.148 Uiso 1 1 calc R U . . . C14 C 0.7770(3) 0.6020(5) 0.4411(2) 0.1288(18) Uani 1 1 d . . . . . H14A H 0.802643 0.582595 0.489281 0.155 Uiso 1 1 calc R U . . . H14B H 0.840429 0.637097 0.423120 0.155 Uiso 1 1 calc R U . . . C16 C 0.4585(3) 0.8865(5) 0.1415(2) 0.1369(18) Uani 1 1 d . . . . . H16A H 0.382818 0.860561 0.146562 0.164 Uiso 1 1 calc R U . . . H16B H 0.456055 0.910938 0.094046 0.164 Uiso 1 1 calc R U . . . C18 C 0.6742(3) 0.4066(3) 0.2930(2) 0.1085(15) Uani 1 1 d . . . . . H18A H 0.599828 0.382681 0.301425 0.130 Uiso 1 1 calc R U . . . H18B H 0.725255 0.335318 0.305466 0.130 Uiso 1 1 calc R U . . . N1 N 0.54392(18) 0.7131(2) 0.30122(11) 0.0682(7) Uani 1 1 d . . . . . H1C H 0.560368 0.662794 0.268281 0.082 Uiso 1 1 calc R U . . . H1D H 0.589161 0.694261 0.340840 0.082 Uiso 1 1 calc R U . . . H1E H 0.554266 0.793824 0.290525 0.082 Uiso 1 1 calc R U . . . N2 N 0.3572(3) 0.3147(3) 0.3550(2) 0.1367(14) Uani 1 1 d . . . . . C2 C 0.3382(3) 0.3541(4) 0.2933(2) 0.1243(16) Uani 1 1 d . . . . . H2 H 0.307866 0.297059 0.258856 0.149 Uiso 1 1 calc R U . . . C3 C 0.4015(2) 0.5609(3) 0.32353(15) 0.0745(9) Uani 1 1 d . . . . . C7 C 0.4202(3) 0.5184(4) 0.38931(17) 0.0990(13) Uani 1 1 d . . . . . H7 H 0.449022 0.572854 0.425299 0.119 Uiso 1 1 calc R U . . . C13 C 0.4252(3) 0.6938(3) 0.30786(19) 0.0966(12) Uani 1 1 d . . . . . H13A H 0.376113 0.718507 0.265331 0.116 Uiso 1 1 calc R U . . . H13B H 0.407930 0.748159 0.344112 0.116 Uiso 1 1 calc R U . . . C15 C 0.3599(3) 0.4768(4) 0.27427(19) 0.1070(14) Uani 1 1 d . . . . . H15 H 0.345997 0.500643 0.228281 0.128 Uiso 1 1 calc R U . . . C17 C 0.3965(4) 0.3960(4) 0.4019(2) 0.1319(17) Uani 1 1 d . . . . . H17 H 0.409351 0.368846 0.447376 0.158 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.1139(7) 0.0819(6) 0.0842(5) -0.0104(5) 0.0181(5) -0.0024(6) F1 0.182(3) 0.347(3) 0.461(4) -0.286(2) 0.126(2) -0.045(3) F2 0.478(5) 0.281(3) 0.206(3) 0.008(3) 0.057(3) -0.256(3) F3 0.496(5) 0.268(3) 0.190(3) 0.101(2) -0.059(3) -0.242(3) F4 0.333(3) 0.170(3) 0.500(5) -0.028(4) -0.296(3) 0.023(3) F5 0.186(3) 0.190(3) 0.388(5) -0.017(4) -0.115(3) 0.032(3) F6 0.411(4) 0.372(4) 0.318(2) -0.241(2) 0.243(2) -0.134(3) O1 0.0906(14) 0.0839(14) 0.0998(14) 0.0129(13) 0.0099(12) 0.0168(12) O2 0.1238(17) 0.0922(16) 0.1364(18) 0.0390(14) 0.0437(14) 0.0311(14) O3 0.0936(14) 0.1187(18) 0.0697(12) 0.0032(13) 0.0032(11) -0.0074(14) O4 0.1390(19) 0.0889(15) 0.1021(14) -0.0197(13) 0.0428(13) -0.0016(15) O5 0.0966(14) 0.1066(16) 0.0784(12) -0.0196(12) 0.0241(10) -0.0068(13) O6 0.0852(14) 0.144(2) 0.0744(12) 0.0188(14) 0.0001(11) -0.0061(15) C1 0.159(3) 0.079(2) 0.207(4) 0.017(3) 0.069(3) 0.040(2) C4 0.114(3) 0.129(3) 0.108(2) 0.042(2) 0.013(2) 0.038(2) C5 0.165(3) 0.118(3) 0.101(2) -0.047(2) 0.050(2) -0.047(3) C6 0.121(3) 0.150(3) 0.0783(19) -0.030(2) 0.0325(18) -0.033(3) C8 0.118(3) 0.138(3) 0.131(3) 0.071(2) 0.019(2) 0.041(3) C9 0.185(4) 0.099(3) 0.176(4) -0.021(3) 0.082(3) 0.027(3) C10 0.105(2) 0.101(3) 0.138(3) -0.044(2) 0.033(2) -0.003(2) C11 0.100(2) 0.195(4) 0.0624(18) 0.002(2) 0.0011(18) -0.027(3) C12 0.137(3) 0.163(4) 0.0677(19) -0.012(2) 0.012(2) -0.054(3) C14 0.100(3) 0.184(4) 0.091(2) 0.018(3) -0.012(2) 0.022(3) C16 0.099(3) 0.206(4) 0.101(2) 0.064(3) 0.005(2) 0.021(3) C18 0.098(2) 0.073(2) 0.156(3) 0.000(2) 0.026(2) 0.014(2) N1 0.0756(13) 0.0657(14) 0.0639(12) 0.0039(11) 0.0143(10) 0.0056(12) N2 0.121(2) 0.091(2) 0.215(3) -0.002(2) 0.074(2) -0.0119(19) C2 0.090(2) 0.130(3) 0.158(3) -0.048(3) 0.037(2) -0.024(2) C3 0.0641(15) 0.0772(19) 0.0861(17) -0.0025(16) 0.0245(13) 0.0038(15) C7 0.112(2) 0.100(3) 0.092(2) -0.003(2) 0.0346(18) -0.002(2) C13 0.0758(18) 0.091(2) 0.129(2) 0.026(2) 0.0346(17) 0.0191(18) C15 0.082(2) 0.143(3) 0.098(2) -0.006(2) 0.0221(18) -0.005(2) C17 0.162(3) 0.110(3) 0.137(3) 0.032(2) 0.063(2) 0.005(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 P1 F5 82.8(2) . . ? F2 P1 F1 93.1(3) . . ? F2 P1 F3 179.2(3) . . ? F2 P1 F5 94.7(2) . . ? F3 P1 F1 86.7(2) . . ? F3 P1 F5 84.6(2) . . ? F4 P1 F1 96.5(3) . . ? F4 P1 F2 85.4(3) . . ? F4 P1 F3 95.4(3) . . ? F4 P1 F5 179.2(3) . . ? F6 P1 F1 176.8(3) . . ? F6 P1 F2 83.7(3) . . ? F6 P1 F3 96.4(3) . . ? F6 P1 F4 83.8(3) . . ? F6 P1 F5 97.0(3) . . ? C4 O1 C18 113.0(3) . . ? C8 O2 C1 113.0(3) . . ? C14 O3 C12 112.8(3) . . ? C9 O4 C5 111.2(3) . . ? C10 O5 C6 112.8(3) . . ? C16 O6 C11 111.7(3) . . ? O2 C1 H1A 109.6 . . ? O2 C1 H1B 109.6 . . ? O2 C1 C9 110.2(3) . . ? H1A C1 H1B 108.1 . . ? C9 C1 H1A 109.6 . . ? C9 C1 H1B 109.6 . . ? O1 C4 H4A 109.9 . . ? O1 C4 H4B 109.9 . . ? O1 C4 C14 109.0(3) . . ? H4A C4 H4B 108.3 . . ? C14 C4 H4A 109.9 . . ? C14 C4 H4B 109.9 . . ? O4 C5 H5A 110.1 . . ? O4 C5 H5B 110.1 . . ? O4 C5 C12 108.0(3) . . ? H5A C5 H5B 108.4 . . ? C12 C5 H5A 110.1 . . ? C12 C5 H5B 110.1 . . ? O5 C6 H6A 109.8 . . ? O5 C6 H6B 109.8 . . ? O5 C6 C11 109.2(3) . . ? H6A C6 H6B 108.3 . . ? C11 C6 H6A 109.8 . . ? C11 C6 H6B 109.8 . . ? O2 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? O2 C8 C16 110.5(3) . . ? H8A C8 H8B 108.1 . . ? C16 C8 H8A 109.5 . . ? C16 C8 H8B 109.5 . . ? O4 C9 C1 106.0(4) . . ? O4 C9 H9A 110.5 . . ? O4 C9 H9B 110.5 . . ? C1 C9 H9A 110.5 . . ? C1 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? O5 C10 H10A 109.7 . . ? O5 C10 H10B 109.7 . . ? O5 C10 C18 109.7(3) . . ? H10A C10 H10B 108.2 . . ? C18 C10 H10A 109.7 . . ? C18 C10 H10B 109.7 . . ? O6 C11 C6 109.7(3) . . ? O6 C11 H11A 109.7 . . ? O6 C11 H11B 109.7 . . ? C6 C11 H11A 109.7 . . ? C6 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? O3 C12 C5 109.5(3) . . ? O3 C12 H12A 109.8 . . ? O3 C12 H12B 109.8 . . ? C5 C12 H12A 109.8 . . ? C5 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? O3 C14 C4 109.3(3) . . ? O3 C14 H14A 109.8 . . ? O3 C14 H14B 109.8 . . ? C4 C14 H14A 109.8 . . ? C4 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? O6 C16 C8 109.4(3) . . ? O6 C16 H16A 109.8 . . ? O6 C16 H16B 109.8 . . ? C8 C16 H16A 109.8 . . ? C8 C16 H16B 109.8 . . ? H16A C16 H16B 108.2 . . ? O1 C18 C10 109.6(3) . . ? O1 C18 H18A 109.7 . . ? O1 C18 H18B 109.7 . . ? C10 C18 H18A 109.7 . . ? C10 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? H1C N1 H1D 109.5 . . ? H1C N1 H1E 109.5 . . ? H1D N1 H1E 109.5 . . ? C13 N1 H1C 109.5 . . ? C13 N1 H1D 109.5 . . ? C13 N1 H1E 109.5 . . ? C2 N2 C17 117.1(4) . . ? N2 C2 H2 118.1 . . ? N2 C2 C15 123.8(4) . . ? C15 C2 H2 118.1 . . ? C7 C3 C13 120.8(3) . . ? C15 C3 C7 117.0(3) . . ? C15 C3 C13 122.2(3) . . ? C3 C7 H7 120.4 . . ? C17 C7 C3 119.2(3) . . ? C17 C7 H7 120.4 . . ? N1 C13 C3 112.2(3) . . ? N1 C13 H13A 109.2 . . ? N1 C13 H13B 109.2 . . ? C3 C13 H13A 109.2 . . ? C3 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C2 C15 H15 120.6 . . ? C3 C15 C2 118.7(4) . . ? C3 C15 H15 120.6 . . ? N2 C17 C7 124.1(4) . . ? N2 C17 H17 117.9 . . ? C7 C17 H17 117.9 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 F1 1.438(4) . ? P1 F2 1.426(4) . ? P1 F3 1.435(4) . ? P1 F4 1.421(4) . ? P1 F5 1.475(4) . ? P1 F6 1.413(4) . ? O1 C4 1.401(4) . ? O1 C18 1.402(4) . ? O2 C1 1.403(5) . ? O2 C8 1.398(5) . ? O3 C12 1.414(5) . ? O3 C14 1.411(5) . ? O4 C5 1.404(4) . ? O4 C9 1.391(5) . ? O5 C6 1.425(4) . ? O5 C10 1.399(4) . ? O6 C11 1.402(5) . ? O6 C16 1.400(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 C9 1.494(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 C14 1.461(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 C12 1.471(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 C11 1.457(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C16 1.459(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C18 1.459(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? N1 H1C 0.8900 . ? N1 H1D 0.8900 . ? N1 H1E 0.8900 . ? N1 C13 1.467(4) . ? N2 C2 1.271(6) . ? N2 C17 1.287(5) . ? C2 H2 0.9300 . ? C2 C15 1.383(6) . ? C3 C7 1.357(4) . ? C3 C13 1.471(5) . ? C3 C15 1.343(5) . ? C7 H7 0.9300 . ? C7 C17 1.352(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C15 H15 0.9300 . ? C17 H17 0.9300 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C4 C14 O3 67.2(4) . . . . ? O2 C1 C9 O4 63.0(4) . . . . ? O2 C8 C16 O6 -62.4(4) . . . . ? O4 C5 C12 O3 -67.8(4) . . . . ? O5 C6 C11 O6 64.0(4) . . . . ? O5 C10 C18 O1 -59.7(4) . . . . ? C1 O2 C8 C16 -176.6(3) . . . . ? C4 O1 C18 C10 -172.5(3) . . . . ? C5 O4 C9 C1 173.4(3) . . . . ? C6 O5 C10 C18 176.0(3) . . . . ? C8 O2 C1 C9 -178.4(3) . . . . ? C9 O4 C5 C12 -176.2(3) . . . . ? C10 O5 C6 C11 175.0(3) . . . . ? C11 O6 C16 C8 179.3(3) . . . . ? C12 O3 C14 C4 179.2(3) . . . . ? C14 O3 C12 C5 177.4(3) . . . . ? C16 O6 C11 C6 175.6(3) . . . . ? C18 O1 C4 C14 -179.6(3) . . . . ? N2 C2 C15 C3 -1.3(6) . . . . ? C2 N2 C17 C7 -1.2(7) . . . . ? C3 C7 C17 N2 0.5(7) . . . . ? C7 C3 C13 N1 86.2(4) . . . . ? C7 C3 C15 C2 0.5(5) . . . . ? C13 C3 C7 C17 179.4(3) . . . . ? C13 C3 C15 C2 -179.0(3) . . . . ? C15 C3 C7 C17 -0.1(5) . . . . ? C15 C3 C13 N1 -94.4(4) . . . . ? C17 N2 C2 C15 1.7(6) . . . . ?